JP2008525592A5 - - Google Patents
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- JP2008525592A5 JP2008525592A5 JP2007548406A JP2007548406A JP2008525592A5 JP 2008525592 A5 JP2008525592 A5 JP 2008525592A5 JP 2007548406 A JP2007548406 A JP 2007548406A JP 2007548406 A JP2007548406 A JP 2007548406A JP 2008525592 A5 JP2008525592 A5 JP 2008525592A5
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- JP
- Japan
- Prior art keywords
- fluorosurfactant
- exchange resin
- anion exchange
- content
- dispersion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000006185 dispersion Substances 0.000 claims description 11
- 239000003957 anion exchange resin Substances 0.000 claims description 10
- 229920002313 fluoropolymer Polymers 0.000 claims description 7
- 239000004811 fluoropolymer Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 4
- 229910001447 ferric ion Inorganic materials 0.000 claims description 4
- 238000005755 formation reaction Methods 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000002738 chelating agent Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N edta Chemical group OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- BFKJFAAPBSQJPD-UHFFFAOYSA-N Tetrafluoroethylene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 239000004815 dispersion polymerization Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000003797 telogen phase Effects 0.000 description 1
Description
溶融加工性ＴＦＥコポリマーの分散重合は、１種または複数種のコモノマーを初期にバッチに添加すること、および／または重合中に導入することを除いて同様である。加えて、炭化水素などのテロゲンを用いて分子量を制御して意図した目的のためのポリマーの望ましいメルト・フローを達成する。ＰＴＦＥ分散液用に用いる同じ分離濃縮操作をＴＦＥコポリマー分散液に用いることができる。
以下に、本発明の好ましい態様を示す。
［１］ 第二鉄イオンを含有する、安定させた、フッ素系界面活性剤含有水性フルオロポリマー分散液のフッ素系界面活性剤の含量を低減させる方法であって、
前記フッ素系界面活性剤含有水性フルオロポリマー分散液を水酸基型である強塩基性陰イオン交換樹脂と接触させて、フッ素系界面活性剤の含量を所定濃度まで低減させる工程と、
前記フッ素系界面活性剤の含量を低減させた後、前記分散液から前記陰イオン交換樹脂を分離する工程と、
前記陰イオン交換樹脂と接触させる工程の前に、鉄との錯体形成時に少なくとも１０18の平衡定数を有するキレート剤の有効量を添加して、第二鉄イオンの錯体を形成することがスカムの形成を防止するようにする工程と、
を含むことを特徴とする方法。
［２］ 前記キレート剤が、エチレンジアミン四酢酸またはその塩であることを特徴とする［１］に記載の方法。
［３］ 前記エチレンジアミン四酢酸またはその塩が、前記分散液に約２〜約１００ｐｐｍの量で添加されることを特徴とする［２］に記載の方法。
［４］ 前記陰イオン交換樹脂が、ポリマーと第４級アンモニウム基を含む官能基とを含有することを特徴とする［１］に記載の方法。
［５］ 前記フッ素系界面活性剤含有水性フルオロポリマー分散液を陰イオン交換樹脂と接触させる前記工程が、フッ素系界面活性剤の含量を約３００ｐｐｍ以下の所定濃度まで低減させることを特徴とする［１］に記載の方法。
［６］ 前記フッ素系界面活性剤含有水性フルオロポリマー分散液を陰イオン交換樹脂と接触させる前記工程が、フッ素系界面活性剤の含量を約１００ｐｐｍ以下の所定濃度まで低減させることを特徴とする［１］に記載の方法。
［７］ 前記フッ素系界面活性剤含有水性フルオロポリマー分散液を陰イオン交換樹脂と接触させる前記工程が、フッ素系界面活性剤の含量を約５０ｐｐｍ以下の所定濃度まで低減させることを特徴とする［１］に記載の方法。
Dispersion polymerization of melt processable TFE copolymers is similar except that one or more comonomers are initially added to the batch and / or introduced during the polymerization. In addition, telogens such as hydrocarbons are used to control the molecular weight to achieve the desired melt flow of the polymer for the intended purpose. The same separation and concentration procedure used for the PTFE dispersion can be used for the TFE copolymer dispersion.
Below, the preferable aspect of this invention is shown.
[1] A method for reducing the content of a fluorosurfactant in a stabilized fluorosurfactant-containing aqueous fluoropolymer dispersion containing ferric ions,
Contacting the fluorosurfactant-containing aqueous fluoropolymer dispersion with a strongly basic anion exchange resin that is a hydroxyl group type to reduce the content of the fluorosurfactant to a predetermined concentration;
Separating the anion exchange resin from the dispersion after reducing the content of the fluorosurfactant;
Before the step of contacting with the anion exchange resin, an effective amount of a chelating agent having an equilibrium constant of at least 10 18 is added during complex formation with iron to form a complex of ferric ions. A process for preventing formation;
A method comprising the steps of:
[2] The method according to [1], wherein the chelating agent is ethylenediaminetetraacetic acid or a salt thereof.
[3] The method according to [2], wherein the ethylenediaminetetraacetic acid or a salt thereof is added to the dispersion in an amount of about 2 to about 100 ppm.
[4] The method according to [1], wherein the anion exchange resin contains a polymer and a functional group containing a quaternary ammonium group.
[5] The step of bringing the fluorosurfactant-containing aqueous fluoropolymer dispersion into contact with an anion exchange resin reduces the content of the fluorosurfactant to a predetermined concentration of about 300 ppm or less. 1].
[6] The step of bringing the fluorosurfactant-containing aqueous fluoropolymer dispersion into contact with an anion exchange resin reduces the content of the fluorosurfactant to a predetermined concentration of about 100 ppm or less. 1].
[7] The step of bringing the fluorosurfactant-containing aqueous fluoropolymer dispersion into contact with an anion exchange resin reduces the content of the fluorosurfactant to a predetermined concentration of about 50 ppm or less. 1].
Claims (1)
前記フッ素系界面活性剤含有水性フルオロポリマー分散液を水酸基型である強塩基性陰イオン交換樹脂と接触させて、フッ素系界面活性剤の含量を所定濃度まで低減させる工程と、
前記フッ素系界面活性剤の含量を低減させた後、前記分散液から前記陰イオン交換樹脂を分離する工程と、
前記陰イオン交換樹脂と接触させる工程の前に、鉄との錯体形成時に少なくとも１０18の平衡定数を有するキレート剤の有効量を添加して、第二鉄イオンの錯体を形成することがスカムの形成を防止するようにする工程と、
を含むことを特徴とする方法。 A method of reducing the content of a fluorosurfactant in a stabilized fluorosurfactant-containing aqueous fluoropolymer dispersion containing ferric ions, comprising:
Contacting the fluorosurfactant-containing aqueous fluoropolymer dispersion with a strongly basic anion exchange resin that is a hydroxyl group type to reduce the content of the fluorosurfactant to a predetermined concentration;
Separating the anion exchange resin from the dispersion after reducing the content of the fluorosurfactant;
Before the step of contacting with the anion exchange resin, an effective amount of a chelating agent having an equilibrium constant of at least 10 18 is added during complex formation with iron to form a complex of ferric ions. A process for preventing formation;
A method comprising the steps of:
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US63829604P | 2004-12-22 | 2004-12-22 | |
| US60/638,296 | 2004-12-22 | ||
| PCT/US2005/046268 WO2006069109A1 (en) | 2004-12-22 | 2005-12-19 | Process for removing fluorosurfactant from aqueous fluoropolymer dispersions and reducing scum formation |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2008525592A JP2008525592A (en) | 2008-07-17 |
| JP2008525592A5 true JP2008525592A5 (en) | 2009-01-29 |
| JP5017123B2 JP5017123B2 (en) | 2012-09-05 |
Family
ID=36177889
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2007548406A Expired - Fee Related JP5017123B2 (en) | 2004-12-22 | 2005-12-19 | Method for removing fluorosurfactant from aqueous fluoropolymer dispersion and reducing scum formation |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US7619018B2 (en) |
| EP (1) | EP1828260B1 (en) |
| JP (1) | JP5017123B2 (en) |
| CN (1) | CN101087814B (en) |
| DE (1) | DE602005024300D1 (en) |
| WO (1) | WO2006069109A1 (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7619018B2 (en) * | 2004-12-22 | 2009-11-17 | E.I. Du Pont De Nemours And Company | Process for removing fluorosurfactant from aqueous fluoropolymer dispersions and reducing scum formation |
| US20060178472A1 (en) * | 2005-02-10 | 2006-08-10 | Johnson David W | Process for producing low fluorosurfactant-containing aqueous fluoropolymer dispersions with controlled pH |
| US7671111B2 (en) * | 2005-02-10 | 2010-03-02 | E.I. Du Pont De Nemours And Company | Monitoring column breakthrough in a process for removing fluorosurfactant from aqueous fluoropolymer dispersions |
| US20070282044A1 (en) * | 2006-05-31 | 2007-12-06 | Robert John Cavanaugh | Concentrated fluoropolymer dispersions stabilized with anionic polyelectrolyte dispersing agents |
| WO2008026707A1 (en) * | 2006-08-31 | 2008-03-06 | Asahi Glass Company, Limited | Perfluorocarboxylic acid salt and method for producing the same |
| WO2012133655A1 (en) | 2011-03-31 | 2012-10-04 | ダイキン工業株式会社 | Aqueous fluoropolymer dispersion |
| CN105377903B (en) * | 2013-07-18 | 2017-03-29 | 旭硝子株式会社 | The manufacture method of aqueous fluorine-containing polymer dispersion, aqueous fluorine-containing polymer dispersion and fluoropolymer |
| CN104119544B (en) * | 2014-07-10 | 2016-05-18 | 中昊晨光化工研究院有限公司 | The preparation method of the concentrated dispersion liquid of perfluoroethylene-propylene |
| CN111138570B (en) * | 2018-11-05 | 2021-10-19 | 中昊晨光化工研究院有限公司 | Method for treating scum of fluorine-containing dispersion concentrated solution |
Family Cites Families (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2559752A (en) | 1951-03-06 | 1951-07-10 | Du Pont | Aqueous colloidal dispersions of polymers |
| US3488288A (en) * | 1968-03-04 | 1970-01-06 | Peter Strong & Co Inc | Denture cleansers |
| US3882153A (en) | 1969-09-12 | 1975-05-06 | Kureha Chemical Ind Co Ltd | Method for recovering fluorinated carboxylic acid |
| US3704272A (en) | 1970-09-15 | 1972-11-28 | Du Pont | Concentration of polytetrafluoroethylene aqueous dispersion |
| DE2903981A1 (en) | 1979-02-02 | 1980-08-07 | Hoechst Ag | RECOVERY OF FLUORINATED EMULGATOR ACIDS FROM BASIC ANION EXCHANGERS |
| JPH01153509A (en) * | 1987-12-11 | 1989-06-15 | Tokai Denka Kogyo Kk | Production of high-purity hydrogen peroxide |
| JP3346090B2 (en) | 1995-03-31 | 2002-11-18 | ダイキン工業株式会社 | Polytetrafluoroethylene aqueous dispersion composition and use thereof |
| US5955556A (en) * | 1995-11-06 | 1999-09-21 | Alliedsignal Inc. | Method of manufacturing fluoropolymers |
| DE19857111A1 (en) * | 1998-12-11 | 2000-06-15 | Dyneon Gmbh | Aqueous dispersions of fluoropolymers |
| DE19933696A1 (en) * | 1999-07-17 | 2001-01-18 | Dyneon Gmbh | Process for the recovery of fluorinated emulsifiers from aqueous phases |
| US6693164B2 (en) | 2000-06-01 | 2004-02-17 | 3M Innovative Properties Company | High purity fluoropolymers |
| US7168617B2 (en) * | 2000-06-07 | 2007-01-30 | Walker Digital, Llc | Game presentation in a retail establishment |
| US6720437B2 (en) * | 2001-02-07 | 2004-04-13 | E. I. Du Pont De Nemours And Company | Fluorinated carboxylic acid recovery and reuse |
| US20030125421A1 (en) * | 2001-08-03 | 2003-07-03 | Hermann Bladel | Aqueous dispersions of fluoropolymers |
| US7279522B2 (en) | 2001-09-05 | 2007-10-09 | 3M Innovative Properties Company | Fluoropolymer dispersions containing no or little low molecular weight fluorinated surfactant |
| CN1326913C (en) | 2002-01-04 | 2007-07-18 | 纳幕尔杜邦公司 | Concentrated fluoroploymer dispersions |
| US6833414B2 (en) | 2002-02-12 | 2004-12-21 | Arkema Inc. | Cross-linkable aqueous fluoropolymer based dispersions containing silanes |
| DE60214343T2 (en) * | 2002-05-22 | 2007-03-29 | 3M Innovative Properties Co., Saint Paul | Process for reducing the content of fluorinated emulsifiers in aqueous fluoropolymer dispersions |
| EP1441014A1 (en) | 2003-01-22 | 2004-07-28 | 3M Innovative Properties Company | Aqueous fluoropolymer dispersion comprising a melt processible fluoropolymer and having a reduced amount of fluorinated surfactant |
| EP1452571B1 (en) | 2003-02-28 | 2005-08-17 | 3M Innovative Properties Company | Fluoropolymer dispersion containing no or little low molecular weight fluorinated surfactant |
| US7619018B2 (en) * | 2004-12-22 | 2009-11-17 | E.I. Du Pont De Nemours And Company | Process for removing fluorosurfactant from aqueous fluoropolymer dispersions and reducing scum formation |
-
2005
- 2005-12-02 US US11/292,455 patent/US7619018B2/en not_active Expired - Fee Related
- 2005-12-19 JP JP2007548406A patent/JP5017123B2/en not_active Expired - Fee Related
- 2005-12-19 CN CN2005800441817A patent/CN101087814B/en not_active Expired - Fee Related
- 2005-12-19 WO PCT/US2005/046268 patent/WO2006069109A1/en active Application Filing
- 2005-12-19 EP EP05854908A patent/EP1828260B1/en not_active Not-in-force
- 2005-12-19 DE DE602005024300T patent/DE602005024300D1/en active Active
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